CN106630679A - Method for preparing wear-resistant superhydrophilic underwater super oleophobic surface on basis of swelling method - Google Patents
Method for preparing wear-resistant superhydrophilic underwater super oleophobic surface on basis of swelling method Download PDFInfo
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- CN106630679A CN106630679A CN201710016890.9A CN201710016890A CN106630679A CN 106630679 A CN106630679 A CN 106630679A CN 201710016890 A CN201710016890 A CN 201710016890A CN 106630679 A CN106630679 A CN 106630679A
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- wear
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- under water
- inorganic particulate
- swelling
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- 238000000034 method Methods 0.000 title claims abstract description 75
- 230000008961 swelling Effects 0.000 title claims abstract description 32
- 238000000576 coating method Methods 0.000 claims abstract description 115
- 239000011248 coating agent Substances 0.000 claims abstract description 113
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 129
- 239000000758 substrate Substances 0.000 claims description 48
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 40
- 239000000853 adhesive Substances 0.000 claims description 39
- 230000001070 adhesive effect Effects 0.000 claims description 39
- 239000004677 Nylon Substances 0.000 claims description 36
- 229920001778 nylon Polymers 0.000 claims description 36
- 230000005660 hydrophilic surface Effects 0.000 claims description 24
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 20
- 235000019253 formic acid Nutrition 0.000 claims description 20
- 239000002245 particle Substances 0.000 claims description 16
- 238000004026 adhesive bonding Methods 0.000 claims description 12
- 238000007654 immersion Methods 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 11
- 229910052681 coesite Inorganic materials 0.000 claims description 7
- 229910052906 cristobalite Inorganic materials 0.000 claims description 7
- 238000000605 extraction Methods 0.000 claims description 7
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- 229910052682 stishovite Inorganic materials 0.000 claims description 7
- 229910052905 tridymite Inorganic materials 0.000 claims description 7
- 229920002302 Nylon 6,6 Polymers 0.000 claims description 5
- 238000003618 dip coating Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 229920002292 Nylon 6 Polymers 0.000 claims description 4
- 239000003822 epoxy resin Substances 0.000 claims description 4
- 229920000647 polyepoxide Polymers 0.000 claims description 4
- 229920000642 polymer Polymers 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Inorganic materials [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000004814 polyurethane Substances 0.000 claims description 3
- 229920003189 Nylon 4,6 Polymers 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 229920005749 polyurethane resin Polymers 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 17
- 239000003292 glue Substances 0.000 abstract description 10
- 238000005507 spraying Methods 0.000 abstract description 10
- 239000010954 inorganic particle Substances 0.000 abstract description 4
- 239000003973 paint Substances 0.000 abstract description 4
- 238000002791 soaking Methods 0.000 abstract description 3
- 239000003921 oil Substances 0.000 description 11
- 238000012360 testing method Methods 0.000 description 11
- 244000137852 Petrea volubilis Species 0.000 description 7
- 238000005299 abrasion Methods 0.000 description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical group [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000011236 particulate material Substances 0.000 description 4
- 230000035939 shock Effects 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 239000012790 adhesive layer Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000000017 hydrogel Substances 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 125000003368 amide group Chemical group 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 238000010422 painting Methods 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 229960002668 sodium chloride Drugs 0.000 description 2
- 235000002639 sodium chloride Nutrition 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- WSLDOOZREJYCGB-UHFFFAOYSA-N 1,2-Dichloroethane Chemical group ClCCCl WSLDOOZREJYCGB-UHFFFAOYSA-N 0.000 description 1
- PXFBZOLANLWPMH-UHFFFAOYSA-N 16-Epiaffinine Natural products C1C(C2=CC=CC=C2N2)=C2C(=O)CC2C(=CC)CN(C)C1C2CO PXFBZOLANLWPMH-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000003486 chemical etching Methods 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000003851 corona treatment Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000010041 electrostatic spinning Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 230000004807 localization Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 description 1
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
- C03C17/38—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal at least one coating being a coating of an organic material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/18—Processes for applying liquids or other fluent materials performed by dipping
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
- B05D5/08—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain an anti-friction or anti-adhesive surface
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2401/00—Form of the coating product, e.g. solution, water dispersion, powders or the like
- B05D2401/10—Organic solvent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2505/00—Polyamides
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Laminated Bodies (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
Abstract
The invention provides a method for preparing a wear-resistant superhydrophilic underwater super oleophobic surface on the basis of a swelling method, and relates to a preparation method of a wear-resistant superhydrophilic underwater super oleophobic coating. The method aims at solving the problems that the existing preparation process of the superhydrophilic underwater super oleophobic surface is complicated, and the wear-resistant performance is poor. The method comprises the following steps of 1, preparing inorganic particle paint; 2, spraying and coating a glue layer; 3, soaking and coating inorganic particle paint, and completing the method for preparing the wear-resistant superhydrophilic underwater super oleophobic surface on the basis of the swelling method. The method provided by the invention belongs to the method for preparing the wear-resistant superhydrophilic underwater super oleophobic surface on the basis of the swelling method.
Description
Technical field
The present invention relates to a kind of preparation method of wear-resisting super hydrophilic super oleophobic coating under water.
Background technology
Ultra-hydrophilic surface due in antifog, automatically cleaning, strengthening the field such as boiling heat transfer and water-oil separating and have important application,
Extensively synthesized and be applied to different substrate materials in recent years.For most of ultra-hydrophilic surfaces, because surface is to the strong affine of water
Power, it also shows that under water height oleophobic or superoleophobic characteristic.However, the method that tradition prepares ultra-hydrophilic surface is adopted mostly
The hydrophilic material of bad mechanical strength is deposited with surface chemical modification or on surface.Such as it is published in Advanced Materials
The 23rd phase of the upper 2011 year article of page 4270《A novel superhydrophilic and underwater
superoleophobic hydrogel-coated mesh for oil/water separation》Describe a kind of super close
The preparation method of water superoleophobic stainless (steel) wire under water, by the way that hydrophilic hydrogel is wrapped on stainless (steel) wire, so that not
Rust steel mesh obtains super hydrophilic property superoleophobic under water, and is applied to water-oil separating, but hydrogel mechanical strength used is poor,
Expand after water suction and soften, be not suitable for large-scale application.It is published in the phase Advanced Materials upper 2013 year the 25th
The article of page 4192《Nanowire-haired inorganic membranes with superhydrophilicity and
underwater ultralow adhesive superoleophobicity for high-efficiency oil/water
separation》Nanowire is etched on copper mesh using the method for chemical etching, it is super hydrophilic superoleophobic under water so as to obtain
Copper mesh, can be used to separate emulsion oil-in-water, though not inquiring into the mechanical strength of copper mesh in text, copper mesh is micro- from text
See its mechanical strength knowable in structure still limited, it is impossible to bear larger external force abrasion.Other technologies such as electrostatic spinning, electricity
Not only preparation technology is loaded down with trivial details for chemical polymerization, corona treatment and template etc., and is difficult to obtain wear-resisting ultra-hydrophilic surface.
Therefore, seek simple, pervasive method is prepared the super hydrophilic superoleophobic under water surface of highly abrasion-resistant and is still difficult at present.
The content of the invention
The invention solves the problems that existing super hydrophilic surface preparation technology superoleophobic under water is loaded down with trivial details and the problem that wears no resistance, and
A kind of method for preparing wear-resisting super hydrophilic surface superoleophobic under water based on swelling method is provided.
A kind of method for preparing wear-resisting super hydrophilic surface superoleophobic under water based on swelling method is completed according to the following steps：
First, inorganic particulate coating is prepared：
By nylon, hydrophilic inorganic particulate and the mixing of formic acid that mass percent is 88%, obtain being applied containing inorganic particulate
Material；
Described nylon is 1 with the mass ratio of hydrophilic inorganic particulate:(0.5～20)；Described applies containing inorganic particulate
The gross mass percentage of nylon and hydrophilic inorganic particulate is 10%～55% in material；
2nd, glue-line is sprayed：
By adhesive even application in substrate surface, uniform glue-line is obtained, then drying is fully cured to glue-line, obtains
The substrate of gluing；
Described adhesive is can be by the swelling adhesive of formic acid or can be by the swelling polymer of formic acid；
3rd, dip-coating inorganic particulate coating：
By the substrate vertical immersion of gluing in coating containing inorganic particulate, soak time is 5s～2h, after then soaking
Substrate extraction is lifted from coating containing inorganic particulate with the speed of 1mm/s～10mm/s, obtain being adsorbed with the substrate of coating, will
It is adsorbed with the substrate of coating and is placed in temperature to be dried in 20 DEG C～80 DEG C baking ovens, until solvent volatilizees completely, that is, completes based on molten
The method that swollen method prepares wear-resisting super hydrophilic surface superoleophobic under water.
The invention has the beneficial effects as follows：
1st, the method for the present invention is simple, is not required to by complicated equipment, and raw material is easy to get, and time-consuming short, reaction condition is gentle, poison
Property is little.
2nd, prepared wear-resisting super hydrophilic super oleophobic coating under water has super hydrophilic characteristic superoleophobic under water：Coating is in air
In to the contact angle of water be 0 °, under water 150 ° are more than to the contact angle of oil, slide angle is less than 10 °.
3rd, prepared wear-resisting super hydrophilic super oleophobic coating under water has excellent mechanical stability.Prepared by the method resistance to
The super hydrophilic surface superoleophobic under water of mill overcomes the defect of the super-hydrophilic coating mechanical stability difference of conventional preparation, substantially increases
The mechanical life of coating, it is with a wide range of applications.
The mechanical stability of coating depends on two aspects：One is the bond strength of coating and substrate, and two is coating itself
Mechanical strength.
Nylon has good mechanical strength, hardness, dimensional stability, toughness and wearability, thus is used to improve painting
The performance of layer.Amido link (- CO-NH-) in nylon produces strong hydrogen bond with the hydroxyl (- OH) of hydrophilic surface of inorganic particles
Effect, so that the particle in coating is firmly bonded together, and improves the mechanical strength of coating.In addition, coating sheet
Also there is very strong adhesion between body and substrate, this adhesion comes from nylon molecules chain and entangles with the physics of adhesive molecule interchain
Twine effect：When the substrate for scribbling adhesive is immersed in coating containing inorganic particulate, formic acid causes adhesive swelling of paint coating, makes
The space obtained between adhesive strand gradually increases.The increase of molecule interchain voids allows nylon molecules to take this opportunity to penetrate into
In these spaces, and there is irregular intertexture with adhesive strand.After formic acid volatilizees completely, nylon molecules and adhesive
It is intermolecular just to form physical entanglement, so as to obtain high bond strength.The mechanical strength of coating itself and its between substrate
High adhesion allows prepared coating to resist the mechanical damage of complexity.
In addition, because coating also has certain thickness and continuous coarse structure, when surface is worn and torn, receive
The coating shedding of damage simultaneously exposes the coating of subordinate, exposed coating there is the roughness consistent with original coating surface, because
And coating can undergo abrasion repeatedly and maintain superoleophobic property under water.
Description of the drawings
Fig. 1 is the SEM figures that the substrate surface of gluing in the step 2 of embodiment one amplifies 8000 times；
Fig. 2 is the SEM figures that wear-resisting super hydrophilic superoleophobic under water slide surface prepared by embodiment one amplifies 2500 times；
Fig. 3 is the SEM figures that wear-resisting super hydrophilic superoleophobic under water slide cross section prepared by embodiment one amplifies 400 times；
Fig. 4 is the SEM figures that wear-resisting super hydrophilic superoleophobic under water slide cross section prepared by embodiment one amplifies 5000 times,
1 is adhesive；
Fig. 5 is the contact angle of the wear-resisting super hydrophilic superoleophobic under water slide surface that water droplet is prepared in embodiment one；
Fig. 6 is the contact angle under water of the wear-resisting super hydrophilic superoleophobic under water slide surface that oil droplet is prepared in embodiment one；
Fig. 7 is the prior slide and the reality with water-wet without glue spraying process prepared with the contrast test one of water-wet
The photo of the wear-resisting super hydrophilic superoleophobic under water slide of the preparation of example one is applied, A is the prior without glue spraying of the preparation of contrast test one
The slide of process, B is wear-resisting super hydrophilic superoleophobic under water slide prepared by embodiment one；
Fig. 8 is the prior slide and the reality with water-wet without glue spraying process prepared with the contrast test one of water-wet
The wear-resisting super hydrophilic superoleophobic under water slide surface of the preparation of example one is applied in the photo after finger friction, A is contrast test
The one prior slide without glue spraying process for preparing, B is wear-resisting super hydrophilic superoleophobic under water slide prepared by embodiment one；
Fig. 9 is the wear-resisting super hydrophilic superoleophobic under water slide surface of the preparation of embodiment one through 24kPa pressure and 600
Contact angle oily under water and slide angle change during mesh Sandpapering different distance, 1 is contact angle, and 2 is slide angle；
Figure 10 is that wear-resisting super hydrophilic superoleophobic under water slide surface prepared by the embodiment one being spontaneously wet out by water is being passed through
Contact angle oily under water and slide angle change when 24kPa pressure and 600 mesh Sandpapering different distance, 1 is contact angle, and 2 are
Slide angle；
Figure 11 is the wear-resisting super hydrophilic superoleophobic under water slide surface for preparing of embodiment one through flow velocity 3.5m/s and straight
The photo that the water column of footpath 5mm is washed away after 1h, 1 is water column shock zone；
Figure 12 is that wear-resisting super hydrophilic super oleophobic coating under water prepared by embodiment one passes through stream with the intersection of adhesive layer
The photo that the water column of fast 3.5m/s and diameter 5mm is washed away after 1h, 1 is water column shock zone；
Figure 13 is that wear-resisting super hydrophilic superoleophobic under water slide surface prepared by embodiment one is passing through different physics and change
Learn contact angle oily under water and slide angle after environmental treatment, " ■ " is contact angle, " ◆ " is slide angle, it in temperature is -30 that a is
DEG C air in process 72h；B is to process 72h in the air that temperature is 100 DEG C；C is in the deionized water that temperature is 80 DEG C
Process 12 hours；D is to process 72h in the aqueous sulfuric acid of pH=1；E is sodium-chloride water solution that mass percent is 3.5%
Middle process 72h；F is soak at room temperature 72h in toluene；G is soak at room temperature 72h in ethanol.
Specific embodiment
Specific embodiment one：Present embodiment is a kind of to prepare wear-resisting super hydrophilic surface superoleophobic under water based on swelling method
Method is completed according to the following steps：
First, inorganic particulate coating is prepared：
By nylon, hydrophilic inorganic particulate and the mixing of formic acid that mass percent is 88%, obtain being applied containing inorganic particulate
Material；
Described nylon is 1 with the mass ratio of hydrophilic inorganic particulate:(0.5～20)；Described applies containing inorganic particulate
The gross mass percentage of nylon and hydrophilic inorganic particulate is 10%～55% in material；
2nd, glue-line is sprayed：
By adhesive even application in substrate surface, uniform glue-line is obtained, then drying is fully cured to glue-line, obtains
The substrate of gluing；
Described adhesive is can be by the swelling adhesive of formic acid or can be by the swelling polymer of formic acid；
3rd, dip-coating inorganic particulate coating：
By the substrate vertical immersion of gluing in coating containing inorganic particulate, soak time is 5s～2h, after then soaking
Substrate extraction is lifted from coating containing inorganic particulate with the speed of 1mm/s～10mm/s, obtain being adsorbed with the substrate of coating, will
It is adsorbed with the substrate of coating and is placed in temperature to be dried in 20 DEG C～80 DEG C baking ovens, until solvent volatilizees completely, that is, completes based on molten
The method that swollen method prepares wear-resisting super hydrophilic surface superoleophobic under water.
The beneficial effect of present embodiment is：1st, the method for present embodiment is simple, is not required to by complicated equipment, raw material
It is easy to get, time-consuming short, reaction condition is gentle, small toxicity.
2nd, prepared wear-resisting super hydrophilic super oleophobic coating under water has super hydrophilic characteristic superoleophobic under water：Coating is in air
In to the contact angle of water be 0 °, under water 150 ° are more than to the contact angle of oil, slide angle is less than 10 °.
3rd, prepared wear-resisting super hydrophilic super oleophobic coating under water has excellent mechanical stability.Prepared by the method resistance to
The super hydrophilic surface superoleophobic under water of mill overcomes the defect of the super-hydrophilic coating mechanical stability difference of conventional preparation, substantially increases
The mechanical life of coating, it is with a wide range of applications.
The mechanical stability of coating depends on two aspects：One is the bond strength of coating and substrate, and two is coating itself
Mechanical strength.
Nylon has good mechanical strength, hardness, dimensional stability, toughness and wearability, thus is used to improve painting
The performance of layer.Amido link (- CO-NH-) in nylon produces strong hydrogen bond with the hydroxyl (- OH) of hydrophilic surface of inorganic particles
Effect, so that the particle in coating is firmly bonded together, and improves the mechanical strength of coating.In addition, coating sheet
Also there is very strong adhesion between body and substrate, this adhesion comes from nylon molecules chain and entangles with the physics of adhesive molecule interchain
Twine effect：When the substrate for scribbling adhesive is immersed in coating containing inorganic particulate, formic acid causes adhesive swelling of paint coating, makes
The space obtained between adhesive strand gradually increases.The increase of molecule interchain voids allows nylon molecules to take this opportunity to penetrate into
In these spaces, and there is irregular intertexture with adhesive strand.After formic acid volatilizees completely, nylon molecules and adhesive
It is intermolecular just to form physical entanglement, so as to obtain high bond strength.The mechanical strength of coating itself and its between substrate
High adhesion allows prepared coating to resist the mechanical damage of complexity.
In addition, because coating also has certain thickness and continuous coarse structure, when surface is worn and torn, receive
The coating shedding of damage simultaneously exposes the coating of subordinate, exposed coating there is the roughness consistent with original coating surface, because
And coating can undergo abrasion repeatedly and maintain superoleophobic property under water.
Specific embodiment two：Present embodiment from unlike specific embodiment one：It is hydrophilic described in step one
Property inorganic particulate be SiO2Particle, TiO2Particle or BaSO4Particle.Other are identical with specific embodiment one.
Specific embodiment three：Present embodiment from unlike specific embodiment one or one of two：Institute in step one
The nylon stated is nylon 6,6, nylon 6 or nylon 4,6..Other are identical with specific embodiment one or two.
Specific embodiment four：Unlike one of present embodiment and specific embodiment one to three：Institute in step 2
The substrate stated is acid resisting material.Other are identical with specific embodiment one to three.
Specific embodiment five：Unlike one of present embodiment and specific embodiment one to four：Institute in step 2
The adhesive stated is adhesive for polyurethane or epoxy resin.Other are identical with specific embodiment one to four.
Specific embodiment six：Unlike one of present embodiment and specific embodiment one to five：Institute in step one
The nylon stated is 1 with the mass ratio of hydrophilic inorganic particulate:4.4.Other are identical with specific embodiment one to five.
Specific embodiment seven：Unlike one of present embodiment and specific embodiment one to six：Institute in step one
The gross mass percentage of nylon and hydrophilic inorganic particulate is 35% in the coating containing inorganic particulate stated.Other be embodied as
Mode one to six is identical.
Specific embodiment eight：Unlike one of present embodiment and specific embodiment one to seven：Will in step 3
In coating containing inorganic particulate, soak time is 10min to the substrate vertical immersion of gluing.Other and specific embodiment one to seven
It is identical.
Specific embodiment nine：Unlike one of present embodiment and specific embodiment one to eight：In step 3 so
Afterwards the substrate after immersion is lifted into extraction with the speed of 2mm/s from coating containing inorganic particulate.Other and specific embodiment one
It is identical to eight.
Specific embodiment ten：Unlike one of present embodiment and specific embodiment one to nine：Will in step 3
It is adsorbed with the substrate of coating and is placed in temperature to be dried in 25 DEG C of baking ovens, until solvent volatilizees completely.Other and specific embodiment
One to nine is identical.
Beneficial effects of the present invention are verified using following examples：
Embodiment one：
A kind of method for preparing wear-resisting super hydrophilic surface superoleophobic under water based on swelling method is completed according to the following steps：
First, inorganic particulate coating is prepared：
By nylon, hydrophilic inorganic particulate and the mixing of formic acid that mass percent is 88%, obtain being applied containing inorganic particulate
Material；
Described nylon is 1 with the mass ratio of hydrophilic inorganic particulate:4.4；Buddhist nun in described coating containing inorganic particulate
The gross mass percentage of imperial and hydrophilic inorganic particulate is 35%；
Described nylon is nylon 6,6；Described hydrophilic inorganic particulate is SiO2Particle；
2nd, glue-line is sprayed：
By adhesive even application in substrate surface, uniform glue-line is obtained, be then dried, until glue-line is fully cured,
Obtain the substrate of gluing；
Described adhesive is the epoxy three-proofing coatings of commercially available Ao Sibang 92；Described substrate is slide；
3rd, dip-coating inorganic particulate coating：
By the substrate vertical immersion of gluing in coating containing inorganic particulate, soak time is 10min, then by after immersion
Substrate lifts extraction with the speed of 2mm/s from coating containing inorganic particulate, obtains being adsorbed with the substrate of coating, will be adsorbed with coating
Substrate be placed in temperature to be dried in 25 DEG C of baking ovens, until solvent volatilizees completely, obtain wear-resisting super hydrophilic load glass superoleophobic under water
Piece.
Contrast test one：
First, inorganic particulate coating is prepared：
By nylon, hydrophilic inorganic particulate and the mixing of formic acid that mass percent is 88%, obtain being applied containing inorganic particulate
Material；
Described nylon is 1 with the mass ratio of hydrophilic inorganic particulate:4.4；Buddhist nun in described coating containing inorganic particulate
The gross mass percentage of imperial and hydrophilic inorganic particulate is 35%；
Described nylon is nylon 6,6；Described hydrophilic inorganic particulate is SiO2Particle；
2nd, dip-coating inorganic particulate coating：
By substrate vertical immersion in coating containing inorganic particulate, soak time is 10min, then by the substrate after immersion with
The speed of 2mm/s lifts extraction from coating containing inorganic particulate, obtains being adsorbed with the substrate of coating, will be adsorbed with the substrate of coating
Temperature is placed in be dried in 25 DEG C of baking ovens, until solvent volatilizees completely, is obtained in advance without the slide of glue spraying process；
Described substrate is slide.
Fig. 1 is the SEM figures that the substrate surface of gluing in the step 2 of embodiment one amplifies 8000 times；As seen from the figure, after solidification
Adhesive coating it is very smooth, without obvious roughness.
Fig. 2 is the SEM figures that wear-resisting super hydrophilic superoleophobic under water slide surface prepared by embodiment one amplifies 2500 times；By
Figure understands that prepared wear-resisting super hydrophilic superoleophobic under water surface is by micron-sized SiO2Particle and less nylon crystal grain group
Into presenting very coarse structure.
Fig. 3 is the SEM figures that wear-resisting super hydrophilic superoleophobic under water slide cross section prepared by embodiment one amplifies 400 times；
As seen from the figure, prepared wear-resisting super hydrophilic super oleophobic coating under water is presented the continuous particle structure piled up, and this causes to work as coating
When being worn, the coating that subordinate exposes still keeps the roughness similar with initial surface, so that the super wetability on surface
It is maintained.
Fig. 4 is the SEM figures that wear-resisting super hydrophilic superoleophobic under water slide cross section prepared by embodiment one amplifies 5000 times,
1 is adhesive；As seen from the figure, it is shown that the friendship of wear-resisting super hydrophilic super oleophobic coating under water, adhesive layer and slide three
Interface.
Fig. 5 is the contact angle of the wear-resisting super hydrophilic superoleophobic under water slide surface that water droplet is prepared in embodiment one；By scheming
Understand, water droplet is presented intimate 0 ° of contact angle on prepared wear-resisting super hydrophilic superoleophobic under water surface, it was demonstrated that its Superhydrophilic.
Fig. 6 is the contact angle under water of the wear-resisting super hydrophilic superoleophobic under water slide surface that oil droplet is prepared in embodiment one；
Described oil droplet is 1,2- dichloroethanes；As seen from the figure, oil droplet under water is in prepared wear-resisting super hydrophilic superoleophobic under water table
Face is presented more than 150 ° of contact angle, it was demonstrated that its superoleophobic property under water.
Fig. 7 is the prior slide and the reality with water-wet without glue spraying process prepared with the contrast test one of water-wet
The photo of the wear-resisting super hydrophilic superoleophobic under water slide of the preparation of example one is applied, A is the prior without glue spraying of the preparation of contrast test one
The slide of process, B is wear-resisting super hydrophilic superoleophobic under water slide prepared by embodiment one；Fig. 8 is with the contrast of water-wet
Prior slide without glue spraying process prepared by test one and with the embodiment one of water-wet prepare it is wear-resisting super hydrophilic under water
In the photo after finger friction, A is the prior without glue spraying process of the preparation of contrast test one to superoleophobic slide surface
Slide, B is wear-resisting super hydrophilic superoleophobic under water slide prepared by embodiment one；Phase is controlled to during finger friction as far as possible
Same dynamics, as seen from the figure, the wear-resisting super hydrophilic super oleophobic coating under water being fixed using adhesive can be resisted well
Finger friction, and the coating fixed without adhesive is easily worn and torn after being spontaneously wet out by water by finger, so that coating shedding, this card
Important function of the clear adhesive in terms of coating stable is maintained.
Prepared by the wear-resisting super hydrophilic superoleophobic under water slide prepared to embodiment one and the embodiment one being spontaneously wet out by water
Wear-resisting super hydrophilic slide surface superoleophobic under water carries out sand paper wear testing；Specifically carry out according to the following steps：To implement
Wear-resisting super hydrophilic superoleophobic under water slide and the embodiment one that is spontaneously wet out by water prepared by example one prepare it is wear-resisting super hydrophilic under water
Superoleophobic slide surface is fixed on desktop (coating is upward) so as to immovable, by the bar shaped sand paper that width is 1cm
Sand face be affixed on by fixed wear-resisting super hydrophilic superoleophobic under water surface, and apply 215g weights on sand paper another side, and
Weight is fixed, friction system (being from top to bottom followed successively by weight, sand paper, wear-resisting super hydrophilic super oleophobic coating under water) is constituted.Line
Property horizontal pulling sand paper make its occur in a localization (1cm × 0.9cm) of ultra-hydrophilic surface it is relative slide it is (manual to pull i.e.
Can, drawing velocity affects little to experimental result, negligible), so as to produce abrasion to surface.Due to sand paper limited length, often
It is secondary with pull 10cm as standard, (1cm × 0.9cm) carries out repeated multiple times pull in identical region.Experimental result is wearing and tearing
The change of contact angle and the slide angle relative wear distance oily under water in region is characterized, and the 10cm that often rubs determines eroded area under water
The contact angle and slide angle of oil.Pressure then enters according to the area of weight 215g and eroded area (1cm × 0.9cm) that apply weight
Row conversion, show that pressure is 24kPa.Described sand paper is 600 mesh.Test result is as shown in FIG. 9 and 10.
Fig. 9 is the wear-resisting super hydrophilic superoleophobic under water slide surface of the preparation of embodiment one through 24kPa pressure and 600
Contact angle oily under water and slide angle change during mesh Sandpapering different distance, 1 is contact angle, and 2 is slide angle；Can by figure
Know, even if prepared wear-resisting super hydrophilic super oleophobic coating under water is after the abrasion (rub every time 10cm) that dry state experiences repeatedly
Its characteristic superoleophobic under water will not be lost, until coating is completely worn out totally, its under water superoleophobic property just lose.
Figure 10 is that wear-resisting super hydrophilic superoleophobic under water slide surface prepared by the embodiment one being spontaneously wet out by water is being passed through
Contact angle oily under water and slide angle change when 24kPa pressure and 600 mesh Sandpapering different distance, 1 is contact angle, and 2 are
Slide angle；As seen from the figure, even if that abrasion repeatedly is experienced under hygrometric state is (every for prepared wear-resisting super hydrophilic super oleophobic coating under water
Secondary friction 10cm) after will not also lose its characteristic superoleophobic under water, until coating is completely worn out totally, its superoleophobic property under water
Just lose.
Figure 11 is the wear-resisting super hydrophilic superoleophobic under water slide surface for preparing of embodiment one through flow velocity 3.5m/s and straight
The photo that the water column of footpath 5mm is washed away after 1h, 1 is water column shock zone；As seen from the figure, prepared super-hydrophilic coating can be fine
Current scour must be resisted.
Figure 12 is that wear-resisting super hydrophilic super oleophobic coating under water prepared by embodiment one passes through stream with the intersection of adhesive layer
The photo that the water column of fast 3.5m/s and diameter 5mm is washed away after 1h, 1 is water column shock zone；As seen from the figure, it is prepared wear-resisting super
The hydrophilic floating coat of super oleophobic coating under water has good bond strength with the junction of adhesive, fine can must resist current punching
Brush.
Figure 13 is that wear-resisting super hydrophilic superoleophobic under water slide surface prepared by embodiment one is passing through different physics and change
Learn contact angle oily under water and slide angle after environmental treatment, " ■ " is contact angle, " ◆ " is slide angle, it in temperature is -30 that a is
DEG C air in process 72h；B is to process 72h in the air that temperature is 100 DEG C；C is in the deionized water that temperature is 80 DEG C
Process 12 hours；D is to process 72h in the aqueous sulfuric acid of pH=1；E is sodium-chloride water solution that mass percent is 3.5%
Middle process 72h；F is soak at room temperature 72h in toluene；G is soak at room temperature 72h in ethanol.As seen from the figure, prepared wear-resisting super parent
Under water superoleophobic surface has good chemical stability to water.
The preparation of the wear-resisting super hydrophilic super oleophobic coating under water of the present embodiment is by carrying out to cured adhesive coating
It is swelling, and fix hydrophilic nylon coatings to realize using the process, adhesive used is the epoxy resin of Ao Sibang 92.So
And, it is in actual applications, any consolidating for nylon/formic acid coating to be can be used in by the swelling adhesive of formic acid or polymer
It is fixed.For example, in addition to epoxy resin, adhesive for polyurethane is equally applicable；And the material such as organic silicon rubber (PDMS), polytetrafluoroethylene (PTFE)
Material cannot be used for fixing nylon coating due to cannot be swelling by formic acid.
The present embodiment coating containing inorganic particulate is by inorganic SiO2Particle, nylon 6,6 and formic acid (88%) three composition, and
In actual applications, each component can be adjusted on demand：Except nylon 6, outside 6, other nylon series of products such as nylon 6, Buddhist nun
Dragon 4,6 etc. is applied to the present invention, here without the need for exhaustive；The concentration of formic acid is heightened also dependent on demand or reduced；Remove
SiO2Outside particle, other particles such as TiO2, BaSO4Also can apply etc. any powder body material that can be used to build coating coarse structure
In the present invention, and its particle size range also can be adjusted in wide scope.
Claims (10)
1. a kind of method that wear-resisting super hydrophilic surface superoleophobic under water is prepared based on swelling method, it is characterised in that one kind is based on swelling
Method prepares the method on wear-resisting super hydrophilic surface superoleophobic under water and completes according to the following steps：
First, inorganic particulate coating is prepared：
By nylon, hydrophilic inorganic particulate and the mixing of formic acid that mass percent is 88%, coating containing inorganic particulate is obtained；
Described nylon is 1 with the mass ratio of hydrophilic inorganic particulate:(0.5～20)；In described coating containing inorganic particulate
The gross mass percentage of nylon and hydrophilic inorganic particulate is 10%～55%；
2nd, glue-line is sprayed：
By adhesive even application in substrate surface, uniform glue-line is obtained, then drying is fully cured to glue-line, obtains gluing
Substrate；
Described adhesive is can be by the swelling adhesive of formic acid or can be by the swelling polymer of formic acid；
3rd, dip-coating inorganic particulate coating：
By the substrate vertical immersion of gluing in coating containing inorganic particulate, soak time is 5s～2h, then by the base after immersion
Bottom lifts extraction with the speed of 1mm/s～10mm/s from coating containing inorganic particulate, obtains being adsorbed with the substrate of coating, will adsorb
The substrate for having coating is placed in temperature to be dried in 20 DEG C～80 DEG C baking ovens, until solvent volatilizees completely, that is, completes based on swelling method
The method for preparing wear-resisting super hydrophilic surface superoleophobic under water.
2. a kind of method that wear-resisting super hydrophilic surface superoleophobic under water is prepared based on swelling method according to claim 1, its
It is characterised by that the hydrophilic inorganic particulate described in step one is SiO2Particle, TiO2Particle or BaSO4Particle.
3. a kind of method that wear-resisting super hydrophilic surface superoleophobic under water is prepared based on swelling method according to claim 1, its
It is characterised by that the nylon described in step one is nylon 6,6, nylon 6 or nylon 4,6.
4. a kind of method that wear-resisting super hydrophilic surface superoleophobic under water is prepared based on swelling method according to claim 1, its
It is characterised by that the substrate described in step 2 is acid resisting material.
5. a kind of method that wear-resisting super hydrophilic surface superoleophobic under water is prepared based on swelling method according to claim 1, its
It is characterised by that the adhesive described in step 2 is adhesive for polyurethane or epoxy resin.
6. a kind of method that wear-resisting super hydrophilic surface superoleophobic under water is prepared based on swelling method according to claim 1, its
The nylon and the mass ratio of hydrophilic inorganic particulate being characterised by described in step one is 1:4.4.
7. a kind of method that wear-resisting super hydrophilic surface superoleophobic under water is prepared based on swelling method according to claim 1, its
The gross mass percentage for being characterised by nylon and hydrophilic inorganic particulate in the coating containing inorganic particulate described in step one is
35%.
8. a kind of method that wear-resisting super hydrophilic surface superoleophobic under water is prepared based on swelling method according to claim 1, its
It is characterised by step 3 that soak time is 10min by the substrate vertical immersion of gluing in coating containing inorganic particulate.
9. a kind of method that wear-resisting super hydrophilic surface superoleophobic under water is prepared based on swelling method according to claim 1, its
It is characterised by step 3 and then the substrate after immersion is lifted into extraction with the speed of 2mm/s from coating containing inorganic particulate.
10. a kind of method that wear-resisting super hydrophilic surface superoleophobic under water is prepared based on swelling method according to claim 1, its
It is characterised by step 3 for the substrate for being adsorbed with coating being placed in temperature to be dried in 25 DEG C of baking ovens, until solvent volatilizees completely.
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